Month: April 2021

Electric Literature of 2698-41-1, Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 2698-41-1, name is 2-(2-Chlorobenzylidene)malononitrile, This compound has unique chemical properties. The synthetic route is as follows.

General procedure: A mixture of hydrazine hydrate (1.5 mmol, 80%),ethyl acetoacetate (1 mmol), aromatic aldehydes (1mmol), malononitrile (1 mmol) and starch solution(4 mL), was stirred at desired temperature for 60-90 min. Progress of the reaction was monitored by TLC. After completion of the reaction, the reaction mixture was cooled to RT and diluted with water. The reaction mixture was filtered for the separation of product. The crude product was purified by recrystallization from ethanol to afford pure products in excellent yield.After removal of the extra added (for work-upprocess) water from the filtered solution, the starchsolution (4 mL) is recovered and reused for thesubsequent reaction.

The chemical industry reduces the impact on the environment during synthesis 2-(2-Chlorobenzylidene)malononitrile. I believe this compound will play a more active role in future production and life.

Application of 23842-82-2, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 23842-82-2 as follows.

General procedure: Matrine 1 (1.24 g, 5 mmol) dissolved in DCM (30 mL) was treatedwith POCl3 (2 eq., 10 mmol) at room temperature. When color of thereaction mixture turned yellow, it was then stirred at 60 C for 2-3 h.The solution was then cooled to room temperature and the correspondinganiline bearing cyan derivatives 18a-h (1-1.5 eq.) dissolvedin DCM were added dropwise, followed by reflux for 12 h at 60C. Afterreaction completion, NaOH aqueous was added to adjust the pH to 8-9.The mixture was then extracted with DCM (3 × 20 mL). The organiclayers were collected, dried over MgSO4, and concentrated. The residuewas purified by column chromatography to obtain product 20a-h.

According to the analysis of related databases, 23842-82-2, the application of this compound in the production field has become more and more popular.

Reference of 6629-04-5, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 6629-04-5 name is N-Cyanoacetylurethane, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

A 2 L, three-neck, round-bottom flask equipped with overhead stirring, a thermocouple, N2 inlet/outlet was charged with Int. 7 (75.0 g, 0.239 mol, 1 wt), acetic acid (600 mL, 8 vol), water (150 mL, 2 vol), and concentrated HC1 (71.3 mL, 0.95 vol). The resulting thin slurry was cooled to 6 C and a solution of NaN02 (16.8 g, 0.243 mol, 1.02 equiv) in water (37.5 mL, 0.5 vol) was added over a period of 10 min while maintaining a batch temperature below 10 C. After an additional 10 min of agitation between 5-10 C,HPLC analysis showed complete conversion of Int. 7 to the diazonium intermediate. A solution of NaOAc (54.5 g, 0.664 mol, 2.78 equiv) in water (225 mL, 3 vol) was added over a period of 6 min while maintaining a batch temperature below 10 C. N-cyanoacetylurethane (37.9 g, 0.243 mol, 1.02 equiv) was immediately added, the cooling was removed, and the batch naturally warmed to 8 C over 35 min. HPLC analysis showed complete consumption of the diazonium intermediate and the reaction was deemed complete. The batch warmed naturally to 21 C and was filtered through Sharkskin filter paper. The reactor and cake were washed sequentially with water (375 mL, 5 vol) twice. The collected orange solid was dried in a 35 C vacuum oven for 64 h to provide crude Int. 8 (104.8 g, 91%). A I L, three-neck, round-bottom flask equipped with overhead stirring, a thermocouple, and N2 inlet/outlet was charged with crude Int. 8 (104.4 g, 1 wt) and acetic acid (522 mL, 5 vol). The resulting slurry was heated to 50 C and held at that temperature for 1.5 h. The batch cooled naturally to 25 C over 2 h and was filtered through Sharkskin filter paper. The reactor and cake were washed sequentially with water (522 mL, 5 vol) and the cake conditioned under vacuum for 1.75 h. The light orange solid was dried to constant weight in a 40 C vacuum oven to provide 89.9 g (78% from Int. 7) of the desired product. 1H NMR (DMSO) was consistent with the assigned structure.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, N-Cyanoacetylurethane, and friends who are interested can also refer to it.

Some common heterocyclic compound, 4210-32-6, name is 4-(tert-Butyl)benzonitrile, molecular formula is C11H13N, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Safety of 4-(tert-Butyl)benzonitrile

General procedure: To a solution of adiponitrile (219 muL, 1.95 mmol) and the appropriate mononitrile (1.30 mmol) in p-xylene (1 mL) in a carousel tube was added t-BuOK (29.2 mg, 0.26 mmol) in one portion. The reaction vessel was heated in a carousel to 120 °C for 4 h. After cooling to room temperature, CH2Cl2 (ca. 30 mL) was used to transfer the mixture onto a silica cartridge for purification.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 4210-32-6, its application will become more common.

127946-77-4, name is 1-Amino-1-cyclopropanecarbonitrile hydrochloride, belongs to nitriles-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Computed Properties of C4H7ClN2

To a vial containing (lR,2R,5S)-2-(2-(ieri-butyl)-5-(4-(l-imino-l- oxidothiomorpholino)phenyl)oxazol-4-yl)-5-fluorocyclohexanecarboxylic acid (12 mg, 0.025 mmol) was added 1-aminocyclopropanecarbonitrile hydrochloride (72.5 mg, 0.61 1 mmol), DIPEA (1 15 uL, 0.696 mmol), and HATU (13.4 mg, 0.035 mmol). The resulting mixture was heated at 65 C for 4.5 hours. The reaction mixture was cooled to RT. The crude mixture was purified directly via reverse phase preparative HPLC (water/10 to 75% MeCN, 0.1 % TFA, 15 min). Fractions with the desired product after HPLC were treated with saturated NaHCC>3 and extracted with CH2CI2 (3 x 10 mL), then EtOAc, washed with brine (30 mL), dried (MgS04), and evaparated under reduced pressure giving 8.2 mg (60%) of (2R,5S)-2-(2-(/er/-butyl)-5-(4-(l-imino-l – oxidothiomorpholino)phenyl)oxazol-4-yl)-N-(l -cyanocyclopropyl)-5- fiuorocyclohexanecarboxamide (Compound 13).1H NMR (500 MHz, CDCl3): delta 0.89-0.84 (m; 2 H); 0.98-0.93 (m; 1 H); 1.33-1.28 (m; 1 H); 1.41-1.39 (m; 1 H); 1.43 (s; 9 H); 2.07-1.92 (m; 3 H); 2.15 (br t; J = 16.14 Hz; 2 H); 2.99 (t; J = 1 1.59 Hz; 1 H); 3.17-3.13 (m; 5 H); 3.94-3.86 (m; 4 H); 5.00 (d; J = 47.85 Hz; 1 H); 6.35 (s; 1 H); 6.95 (d; J = 8.51 Hz; 2 H); 7.46 (d; J = 8.47 Hz; 2 H); MS (ES, m/z): 542.2 (M + 1)

The synthetic route of 127946-77-4 has been constantly updated, and we look forward to future research findings.

Related Products of 915394-29-5,Some common heterocyclic compound, 915394-29-5, name is 2-(3-Aminophenyl)-2-methylpropanenitrile, molecular formula is C10H12N2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

General procedure: 4-methyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl) benzoic acid (8.95g, 31mmol) was stirred in a solvent of 58 dimethyl formamide (25mL).The reaction solution was added with 59 HATU (12.98g, 34.1mmol), 72 DIPEA (10.26mL, 62.0mmol) and 104 3-(trifluoromethyl)aniline (5g, 31mmol), followed by stirring for about 8h at room temperature. The reaction mixture was diluted with ethyl acetate and washed with a saturated aqueous sodium bicarbonate solution and saline. The organic layer thus obtained was dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The resulting mixture was concentrated to give the crude 132 product, which was purified by silica gel column chromatography.

The synthetic route of 915394-29-5 has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 63069-50-1, name is 4-Amino-3-fluorobenzonitrile, molecular formula is C7H5FN2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. SDS of cas: 63069-50-1

Step 8 30.8 g (0.45 mol) of sodium nitrite was added slowly to 244 cm3 of concentrated sulfuric acid while stirring. After the addition was complete, the solution was heated to a temperature of 50 C. to dissolve the crystals. The solution was added drop-wise to 406 cm3 of acetic acid while cooling on an ice water bath and stirring. 55 g (0.40 mol) of 4-amino-3-fluorobenzonitrile was added slowly to maintain the temperature below 25 C. and the mixture was stirred at 25 C. for one hour to dissolve the crystals and form the corresponding diazonium salt. While cooling with ice water and stirring, the diazonium salt was added drop-wise to a solution of 87.4 g (0.61 mol) of copper (I) bromide and 244 cm3 of hydrobromic acid (47%) and allowed to remain overnight at room temperature. The crystals deposited were filtered out, washed with water and recrystallized from hexane to yield 61.7 g (0.31 mol) of 4-bromo-3-fluorobenzonitrile.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 63069-50-1, its application will become more common.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 35202-54-1, name is 4,5-Dimethoxy-1-cyanobenzocyclobutane, A new synthetic method of this compound is introduced below., SDS of cas: 35202-54-1

4,5-Dimethoxy-1-cyanobenzocyclobutane (10 g, 52.85 mmol)Soluble in ammonia-methanol solution (2M, 530ml), replacing nitrogen three times,Then add Raney nickel (1.0g)Replace hydrogen (45psi),The reaction was stirred at 20 °C for 12 h. TLC detection is complete, filtered through diatomaceous earth,The solvent was evaporated to give 4,5-dimethoxy-1-methylaminobenzocyclobutane (10.0 g, 98percent) as an oil.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference of 218632-01-0,Some common heterocyclic compound, 218632-01-0, name is 3-Fluoro-4-nitrobenzonitrile, molecular formula is C7H3FN2O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

The mixture of 16.7 g (100 mmol) of 3-fluoro-4-nitrobenzonitrile and 100 mL of the solution of dimethylamine in ethanol (5 M) was refluxed overnight. The resulting dark red solution was then poured in to 100 mL of ice-water. The precipitate was collected by filtration and washed by H2O (50 mL*2) and ethanol (50 mL*2) to give 16.9 g of a organe needle crystal as the desired product. MS ESI (m/z) 192 (M+1)+.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 3-Fluoro-4-nitrobenzonitrile, its application will become more common.

Reference of 51762-67-5, The chemical industry reduces the impact on the environment during synthesis 51762-67-5, name is 3-Nitrophthalonitrile, I believe this compound will play a more active role in future production and life.

Using 3-nitrophthalonitrile (20 mmol) and sodium p-hydroxybenzenesulfonate (20-70 mmol, preferably 60 mmol) as reactants and dimethyl sulfoxide (40-200 mL, preferably 140 mL) as solvent in carbonic acid Potassium (30 to 90 mmol, preferably 80 mmol) is present and under nitrogen protection, the reaction is stirred at room temperature to 60C (preferably 60C) for 24 to 72 hours and monitored by thin layer chromatography. After the reaction was completed, the reaction solution was poured into ice chloroform to precipitate a yellow-white precipitate, which was filtered, washed with ethanol and acetone until the filtrate was colorless, and dried in vacuum at 50 C. to obtain a pale yellow product with a yield of 92%.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3-Nitrophthalonitrile, other downstream synthetic routes, hurry up and to see.